CN114855045A - High-strength high-toughness high-density multi-component alloy and preparation method thereof - Google Patents
High-strength high-toughness high-density multi-component alloy and preparation method thereof Download PDFInfo
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
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Abstract
The invention discloses a high-strength high-density multi-component alloy and a preparation method thereof, wherein the high-strength high-density multi-component alloy comprises the following components in percentage by atom: 47-58% of W, 8-17% of Mo, 4-6% of V, 14-25% of Fe and 6-15% of Ni. The high-strength high-toughness high-density multi-component alloy provided by the invention has the characteristic of multiphase structure formed by equal matrix with a body-centered cubic structure and other face-centered cubic structures, and the mass density of the alloy is 13.8-17.5 g-cm ‑3 The compressive yield strength at room temperature is 1000-2200 MPa, the ultimate compressive strength is 1800-3200 MPa, and the compressive strain value is more than20 percent, and the Vickers hardness value is 4-12 GPa; can be used as high-performance heavy alloy to be applied to the fields of aerospace, electronic products, national defense science and technology, heavy industry and the like.
Description
Technical Field
The invention belongs to the technical field of metal material preparation, and particularly relates to a high-strength, high-toughness and high-density multi-component alloy and a preparation method thereof.
Background
The high-density alloy also has the characteristics of high strength, high hardness and the like, and is widely applied to the fields of aerospace, electronic products, national defense science and technology, heavy industry and the like. The most common high density alloys at present are tungsten based heavy alloys, which typically comprise more than 80 wt% W element and small amounts of other metal elements such as nickel, iron, copper, etc. The microstructure of tungsten-based heavy alloys is generally composed of a binder phase formed by tungsten grains of relatively large size and elements such as iron and nickel. In recent years, researchers have made many attempts in the aspects of preparation processes and the like to improve the mechanical properties of tungsten-based heavy alloys, but factors such as the inherent coarse tungsten grain structure and the intrinsic brittleness of the tungsten-based heavy alloys often limit further improvement of the mechanical properties of the alloys, and the tungsten-based heavy alloys are difficult to effectively serve in application fields with higher requirements on the properties. Therefore, new high-performance high-density alloys are yet to be developed.
The multi-component High-entropy alloy (High-entropy alloy) comprises at least four or five components, the content of each component is 5 at-35 at%, and the High-entropy alloy can have excellent comprehensive performance through reasonable component design. The multi-component high-entropy alloy concept also has certain potential in the aspect of developing high-performance high-density alloy. For example: hu et al [ X.Hu, X.Liu, D.Yan, Z.Li, J.alloys Compd.894(2021)162505]Report W 35 Ta 35 Mo 10 Nb 10 V 10 (at. -%) high-density high-entropy alloy has mass density of 14.65g cm -3 The microhardness and the ultimate compressive strength can respectively reach 6.50GPa and 2519 MPa. Although the high-entropy alloy has good performances such as high density, high strength and high hardness, Ta contained in the structure thereof 2 VO 6 The brittle phase is not good for the plasticity of the alloy, so that the alloy shows room temperature brittleness. Therefore, the development of high density alloys having high strength, high hardness and high toughness at room temperature still faces technical problems.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made keeping in mind the above and/or other problems occurring in the prior art.
One of the objects of the present invention is to provide a high strength and toughness high density multicomponent alloy exhibiting a multiphase structure characteristic consisting of a matrix of a body-centered cubic structure and other face-centered cubic structures being equal.
In order to solve the technical problems, the invention provides the following technical scheme: a high-strength, high-toughness and high-density multicomponent alloy comprises the following components in atomic percentage: 47-58% of W, 8-17% of Mo, 4-6% of V, 14-25% of Fe and 6-15% of Ni;
wherein the sum of the atomic percentage contents of W, Mo and V is less than or equal to 80 percent and more than or equal to 60 percent; fe. The sum of the atomic percentage contents of Ni is more than or equal to 20 percent and less than or equal to 40 percent; the sum of the atomic percentages of the components is 100 percent.
The invention also aims to provide a preparation method of the high-strength, high-toughness and high-density multicomponent alloy, which comprises the steps of preparing raw materials of each component according to the atomic percentage of the alloy, and sintering under the protection of vacuum or inert gas to obtain the alloy material.
As a preferred scheme of the preparation method of the high-strength, high-toughness and high-density multicomponent alloy, the method comprises the following steps: and the sintering adopts a vacuum hot-pressing sintering or discharge plasma sintering method.
As a preferred scheme of the preparation method of the high-strength, high-toughness and high-density multicomponent alloy, the method comprises the following steps: sintering under a vacuum condition, and maintaining the vacuum degree in the furnace at 1-0.0001 Pa.
As a preferred scheme of the preparation method of the high-strength, high-toughness and high-density multicomponent alloy, the method comprises the following steps: and sintering under the inert gas protection condition, and maintaining the pressure of the inert gas in the furnace at 0.000001-5 MPa.
As a preferred scheme of the preparation method of the high-strength, high-toughness and high-density multicomponent alloy, the method comprises the following steps: and sintering, wherein the sintering temperature is 900-1400 ℃, and the sintering time is 3-30 min.
As a preferred scheme of the preparation method of the high-strength, high-toughness and high-density multicomponent alloy, the method comprises the following steps: the raw materials of each component are pure metal powder with the purity higher than 99 wt.%.
As a preferred scheme of the preparation method of the high-strength, high-toughness and high-density multicomponent alloy, the method comprises the following steps: after the raw materials of each component are prepared, the raw materials of each component are subjected to ball milling in a ball mill for 5-100 hours.
As a preferable scheme of the preparation method of the high-strength, high-toughness and high-density multicomponent alloy, the method comprises the following steps: ball-milling the raw materials of each component in a ball mill, wherein the ball-material ratio during ball milling is 8-13: 1, the rotating speed of the ball mill is 150-600 revolutions per minute, and the ball milling is carried out under the protection of vacuum or inert gas.
As a preferred scheme of the preparation method of the high-strength, high-toughness and high-density multicomponent alloy, the method comprises the following steps: the obtained alloy material has a mass density of 13.8-17.5 g/cm -3 The compressive yield strength is 1000-2200 MPa at room temperature, the ultimate compressive strength is 1800-3200 MPa, the compressive strain value is more than 20%, and the Vickers hardness value is 4-12 GPa.
Compared with the prior art, the invention has the following beneficial effects:
the multi-component high-density alloy material provided by the invention comprises a matrix phase with a body-centered cubic (BCC) structure and a face-centered cubic (FCC) structure phase, and shows a multi-phase composite structure characteristic. The existence of the multi-component alloy elements ensures that the solid solution strengthening effect in the alloy is obvious, and the higher strength is ensured; w, Mo and the existence of V elements ensure the high density characteristic of the alloy and the characteristic that the Body Centered Cubic (BCC) structure is a matrix; the existence of Fe and Ni elements ensures the formation of a face-centered cubic (FCC) structural phase and plays an important role in the plasticity and toughness of the alloy; the excellent obdurability and high density characteristics of the alloy can be applied to the fields of aerospace, electronic products, national defense science and technology, heavy industry and the like.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 is an XRD spectrum of the high-toughness high-density multicomponent alloy material provided by example 1 of the invention.
FIG. 2 is a scanning electron microscope topography of the high-toughness high-density multicomponent alloy material provided in example 1 of the present invention.
FIG. 3 is the EBSD antipole diagram (IPF) and phase distribution diagram of the high-toughness high-density multicomponent alloy material provided in example 1 of the present invention.
FIG. 4 is a scanning electron microscope energy spectrum surface distribution image of the high-toughness high-density multicomponent alloy material provided in example 1 of the present invention.
FIG. 5 is a compression mechanical diagram of the high-strength high-density multicomponent alloy material provided in example 1 of the present invention.
FIG. 6 is an XRD spectrum of the high-toughness high-density multicomponent alloy material provided in example 2 of the present invention.
FIG. 7 is a scanning electron microscope topography of the high-toughness high-density multicomponent alloy material provided in example 2 of the present invention.
FIG. 8 is the EBSD antipole (IPF) and phase distribution diagram of the high-toughness high-density multicomponent alloy material provided in example 2 of the present invention.
FIG. 9 is a compression mechanical diagram of the high-strength high-density multicomponent alloy material provided in example 2 of the present invention.
FIG. 10 is an XRD spectrum of the high-toughness high-density multicomponent alloy material provided in example 3 of the present invention.
FIG. 11 is a scanning electron microscope topography of the high toughness high density multicomponent alloy material provided in example 3 of the present invention.
FIG. 12 is the EBSD antipole (IPF) and phase distribution diagram of the high-toughness high-density multicomponent alloy material provided in example 3 of the present invention.
FIG. 13 is a compression mechanical diagram of the high-strength high-density multicomponent alloy material provided in example 3 of the present invention.
FIG. 14 is an XRD spectrum of the high-toughness high-density multicomponent alloy material provided in example 4 of the present invention.
FIG. 15 is a scanning electron microscope topography of the high-toughness high-density multicomponent alloy material provided in example 4 of the present invention.
FIG. 16 is the EBSD antipole (IPF) and phase distribution diagram of the high-toughness high-density multicomponent alloy material provided in example 4 of the present invention.
FIG. 17 is a compression mechanical diagram of the high-strength high-density multicomponent alloy material provided in example 4 of the present invention.
FIG. 18 is an XRD spectrum of the high-toughness high-density multicomponent alloy material provided by comparative example 1 of the invention.
FIG. 19 is a scanning electron microscope topography of the high toughness high density multicomponent alloy material provided by comparative example 1 of the present invention.
FIG. 20 is an EBSD antipolar diagram (IPF) and phase distribution diagram of the high-toughness high-density multicomponent alloy material provided by comparative example 1 of the present invention.
FIG. 21 is a graph showing the compression mechanics of the high strength, toughness and high density multicomponent alloy material provided in comparative example 1 of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, specific embodiments thereof are described in detail below with reference to examples of the specification.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, the references herein to "one embodiment" or "an embodiment" refer to a particular feature, structure, or characteristic that may be included in at least one implementation of the present invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
According to the chemical formula W 50 Mo 10 V 5 Fe 22.4 Ni 12.6 (atomic percentage) burdening, putting metal powder corresponding to each pure element as a raw material into a ball milling tank filled with grinding balls under the vacuum protection condition, sealing, putting the ball milling tank filled with the metal powder into a ball mill, and operating for 15 hours; the ball-material ratio during ball milling is 10:1, and the rotating speed of the ball mill is 300 revolutions per minute;
then taking out the metal powder under the vacuum protection condition, and putting the metal powder into a sintering grinding tool and compacting the metal powder; sintering the compacted blank by adopting a discharge plasma method under the vacuum protection condition, wherein the sintering temperature is 1250 ℃, and the sintering time is 10 minutes; after sintering, a dense bulk material, i.e. the alloy of example 1, was obtained.
As can be seen from the XRD pattern of FIG. 1, the multicomponent alloy obtained in example 1 consists of a body-centered cubic (BCC) structured matrix, 2 face-centered cubic (FCC) structured phases and a small amount of a V-rich phase of BCC structure. As can be seen from the scanning electron micrograph of FIG. 2 and the EBSD micrograph of FIG. 3, the BCC grains have an average size of 1.73 μm and the BCC matrix phase accounts for about 66%. From the energy spectrum analysis results of fig. 4, the BCC matrix phase is rich in W and Mo, and the FCC1 phase is rich in Fe and Ni; in addition, Mo is enriched in FCC2 phase. As is clear from the compression mechanical graph of fig. 5, the bulk alloy obtained in example 1 has a yield strength of 1255MPa, a compressive strength of 2639MPa, and a compressive strain of 32%, and exhibits excellent toughness.
Example 2
According to the chemical formula W 55 Mo 15 V 5 Fe 16 Ni 9 (atomic percentage) burdening, putting metal powder corresponding to each pure element as a raw material into a ball milling tank filled with grinding balls under the vacuum protection condition, sealing, putting the ball milling tank filled with the metal powder into a ball mill, and operating for 15 hours; the ball-material ratio during ball milling is 10:1, and the rotating speed of the ball mill is 300 revolutions per minute;
then taking out the metal powder under the vacuum protection condition, and putting the metal powder into a sintering grinding tool and compacting the metal powder; sintering the compacted blank by adopting a discharge plasma method under the vacuum protection condition, wherein the sintering temperature is 1250 ℃, and the sintering time is 10 minutes; after sintering, a dense bulk material, i.e. the alloy of example 2, was obtained.
As can be seen from the XRD pattern of FIG. 6, the multicomponent alloy obtained in example 2 consists of a BCC-structured matrix, 2 FCC phases and a small amount of a V-rich phase of BCC structure. As can be seen from the scanning electron micrograph of FIG. 7 and the EBSD micrograph of FIG. 8, the BCC grains have an average size of 2.22 μm and the BCC matrix phase accounts for about 86%. As is clear from the compressive mechanical graph of fig. 9, the bulk alloy obtained in example 2 exhibited excellent toughness with a yield strength of 1208MPa, a compressive strength of 2665MPa, and a compressive strain of 31%.
Example 3
According to the chemical formula W 50 Mo 10 V 5 Fe 22.4 Ni 12.6 (atomic percentage) burdening, putting metal powder corresponding to each pure element as a raw material into a ball milling tank filled with grinding balls under the vacuum protection condition, sealing, putting the ball milling tank filled with the metal powder into a ball mill, and operating for 15 hours; the ball-material ratio during ball milling is 10:1, and the rotating speed of the ball mill is 300 revolutions per minute;
then taking out the metal powder under the vacuum protection condition, and putting the metal powder into a sintering grinding tool and compacting the metal powder; sintering the compacted blank by adopting a discharge plasma method under the vacuum protection condition, wherein the sintering temperature is 1350 ℃, and the sintering time is 10 minutes; after sintering, a dense bulk material, i.e. the alloy of example 3, was obtained.
As can be seen from the XRD pattern of FIG. 10, the multicomponent alloy obtained in example 3 consists of a BCC-structured matrix, 2 FCC phases and a small amount of a V-rich phase of BCC structure. As can be seen from the scanning electron micrograph of FIG. 11 and the EBSD micrograph of FIG. 12, the BCC grains have an average size of 1.78 μm and the BCC matrix phase accounts for about 80%. As is clear from the compression mechanical graph of FIG. 13, the bulk alloy obtained in example 3 exhibited excellent toughness with a yield strength of 1375MPa, a compressive strength of 2839MPa, and a compressive strain of 30%.
Example 4
According to the chemical formula W 55 Mo 15 V 5 Fe 16 Ni 9 (atomic percentage) burdening, putting metal powder corresponding to each pure element as a raw material into a ball milling tank filled with grinding balls under the vacuum protection condition, sealing, putting the ball milling tank filled with the metal powder into a ball mill, and operating for 15 hours; the ball-material ratio during ball milling is 10:1, and the rotating speed of the ball mill is 300 revolutions per minute;
then taking out the metal powder under the vacuum protection condition, and putting the metal powder into a sintering grinding tool and compacting the metal powder; sintering the compacted blank by adopting a discharge plasma method under the vacuum protection condition, wherein the sintering temperature is 1350 ℃, and the sintering time is 5 minutes; after sintering, a dense bulk material, i.e. the alloy of example 4, was obtained.
As can be seen from the XRD pattern of FIG. 14, the multicomponent alloy obtained in example 4 consists of a BCC-structured matrix, 2 FCC phases and a small amount of a V-rich phase of BCC structure. As can be seen from the scanning electron micrograph in FIG. 15 and the EBSD micrograph in FIG. 16, the BCC grains have an average size of 2.20 μm and the BCC matrix phase accounts for about 87%. As is clear from the compressive mechanical graph of fig. 17, the bulk alloy obtained in example 4 exhibited excellent toughness with a yield strength of 1219MPa, a compressive strength of 2272MPa, and a compressive strain of 22%.
Comparative example 1
According to the chemical formula W 50 Mo 10 V 5 Fe 22.4 Ni 12.6 (atomic percentage) burdening, putting metal powder corresponding to each pure element as a raw material into a ball milling tank filled with grinding balls under the vacuum protection condition, sealing, putting the ball milling tank filled with the metal powder into a ball mill, and operating for 15 hours; the ball-material ratio during ball milling is 10:1, and the rotating speed of the ball mill is 300 revolutions per minute;
then taking out the metal powder under the vacuum protection condition, and putting the metal powder into a sintering grinding tool and compacting the metal powder; sintering the compacted blank by adopting a discharge plasma method under the vacuum protection condition, wherein the sintering temperature is 1150 ℃, and the sintering time is 10 minutes; the alloy of comparative example 1 was obtained after sintering.
As can be seen from the XRD pattern of FIG. 18, the multicomponent alloy obtained in comparative example 1 consists of a BCC-structured matrix, 2 FCC phases, and a small amount of a V-rich phase and a small amount of a μ -phase of BCC structure. As can be seen from the scanning electron micrograph in FIG. 19 and the EBSD micrograph in FIG. 20, the BCC grains had an average size of 0.36 μm and the BCC matrix phase accounted for about 42%. As can be seen from the compressive mechanical curve chart of FIG. 21, the bulk alloy obtained in comparative example 1 has poor mechanical properties, a compressive strength of 879MPa, and no yield stage and fracture strain values.
In the multi-component high-density alloy material provided by the invention, the following characteristics are provided in the aspect of component matching: firstly, compared with the traditional tungsten-based high-density alloy, Mo and V elements are introduced into the alloy, and the difference between the atomic radius of Mo and V and the atomic radius of W is utilized, so that larger lattice distortion is generated in a Body Centered Cubic (BCC) matrix structure to block dislocation motion, the solid solution strengthening effect in the alloy is effectively improved, and the strength and the hardness are improved; on the other hand, the introduction of Mo and V elements is beneficial to reducing the ductile-brittle transition temperature of the traditional pure W matrix, reducing the room temperature brittleness and improving the toughness.
The multicomponent high-density alloy material of the invention is introduced with alloying elements such as Fe, Ni and the like, and the comprehensive effect is briefly described as follows: 1) fe and Ni elements promote the formation of a face-centered cubic (FCC) phase, which is beneficial to improving the ductility and toughness; 2) a small amount of Fe and Ni elements are dissolved in a Body Centered Cubic (BCC) matrix in a solid mode, and lattice distortion can be caused in the Body Centered Cubic (BCC) matrix to block dislocation movement, so that the solid solution strengthening effect in the alloy is effectively improved, and the strength of the alloy is further improved.
The multi-component high-density alloy material provided by the invention comprises a matrix phase with a body-centered cubic (BCC) structure and a face-centered cubic (FCC) structure phase, and shows a multi-phase composite structure characteristic. The existence of the multi-component alloy elements ensures that the solid solution strengthening effect in the alloy is obvious, and the higher strength is ensured; w, Mo and the existence of V elements ensure the high density characteristic of the alloy and the characteristic that the Body Centered Cubic (BCC) structure is taken as a matrix; the existence of Fe and Ni elements ensures the formation of a face-centered cubic (FCC) structural phase and plays an important role in the plasticity and toughness of the alloy; the excellent obdurability and high density characteristics of the alloy can be applied to the fields of aerospace, electronic products, national defense science and technology, heavy industry and the like.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (10)
1. A high-strength high-density multicomponent alloy is characterized in that: the composition comprises the following components in atomic percentage: 47-58% of W, 8-17% of Mo, 4-6% of V, 14-25% of Fe and 6-15% of Ni;
wherein the sum of the atomic percentage contents of W, Mo and V is less than or equal to 80 percent and more than or equal to 60 percent; fe. The sum of the atomic percentage contents of Ni is more than or equal to 20 percent and less than or equal to 40 percent; the sum of the atomic percentages of the components is 100 percent.
2. The method for preparing the high-strength high-toughness high-density multi-component alloy according to claim 1, wherein the method comprises the following steps: the method comprises the steps of preparing raw materials of each component according to the atomic percentage of the alloy, and sintering under the protection of vacuum or inert gas to obtain the alloy material.
3. The method for preparing the high-strength high-toughness high-density multi-component alloy according to claim 2, wherein the method comprises the following steps: and the sintering adopts a vacuum hot-pressing sintering or discharge plasma sintering method.
4. The method for preparing the high-strength high-toughness high-density multi-component alloy according to claim 2, wherein the method comprises the following steps: sintering under a vacuum condition, and maintaining the vacuum degree in the furnace at 1-0.0001 Pa.
5. The method for preparing the high-strength high-toughness high-density multi-component alloy according to claim 2, wherein the method comprises the following steps: and sintering under the inert gas protection condition, and maintaining the pressure of the inert gas in the furnace at 0.000001-5 MPa.
6. The method for preparing the high-strength high-toughness high-density multi-component alloy according to any one of claims 2 to 5, wherein the method comprises the following steps: and sintering, wherein the sintering temperature is 900-1400 ℃, and the sintering time is 3-30 min.
7. The method for preparing the high-strength high-toughness high-density multi-component alloy according to claim 6, wherein the method comprises the following steps: the raw materials of each component are pure metal powder with the purity higher than 99 wt.%.
8. The method for preparing the high-strength, high-toughness and high-density multi-component alloy according to any one of claims 2 to 5 and 7, wherein the method comprises the following steps: after the raw materials of each component are prepared, the raw materials of each component are subjected to ball milling in a ball mill for 5-100 hours.
9. The method for preparing the high-strength high-toughness high-density multi-component alloy according to claim 8, wherein the method comprises the following steps: ball-milling the raw materials of each component in a ball mill, wherein the ball-material ratio during ball milling is 8-13: 1, the rotating speed of the ball mill is 150-600 revolutions per minute, and the ball milling is carried out under the protection of vacuum or inert gas.
10. The method for preparing the high-strength high-density multi-component alloy according to any one of claims 2 to 5, 7 and 9, wherein the method comprises the following steps: the obtained alloy material has a mass density of 13.8-17.5 g/cm -3 The compressive yield strength is 1000-2200 MPa at room temperature, the ultimate compressive strength is 1800-3200 MPa, the compressive strain value is more than 20%, and the Vickers hardness value is 4-12 GPa.
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